Process of making auxiliary mordants containing antimony and glycolic acid.



UNITED STATES PATENT OFFICE.

OTTO LIEBKNEGHT, 0F FRANKFORT-ON-THE-MAIN, AND FERDINAND BLUMENTHAL, I

OF WIESBADEN, GERMANY. I

PROCESS OF, MAKING AUXILIARY MORDANTS CONTAINING ANTIMONY AND GLYGOLIG ACID. I

1,059,741. No Drawing.

Specification of Letters Patent.

Application filed October 16, 1911. Serial No. 655,055.

Patented Apr. 22, 1913.

To all whom it may concern: I

Be it known that we, Orro LIEBKNEO'HT and FERDINAND BLUMENTHAL, citizens of the German Empire, and residents, respectively, of Frankfort-on-the Main and Wiesbaden, in said Empire, have invented certain new and useful Improvements in Processes" preparing such salts, various methods may 4 be employed: Aqueoussolutions of glycolic acid are saturated with freshly precipitated or amorphous commercial antimony oxid in the presence of alkalis oralkaline earth-' metals, after which" the solution is evaporated'to dryness or permitted to crystallize at a certain concentration. A sodium salt which contains about 30% of antimony is thus easily obtained. These highly concentrated' salts easily-allow the antimony oxid to precipitate on being dissolved in much water, especially on being-heated. 'Perma nent clear solutions, however, are obtained when free glycolic acid or glycolates are added to the salts. Of course these acid glycolates may be added-from the startfto diiferonly by theircontents of the solutions saturated withantimony, and. i then clear soluble products are "obtained;

even when heated; The-same-result is also obtained when nocompletelsaturation with antimony oxid 1 has '1 taken place Furthermore, antimony oxy-chlorid, such'as is pro-' duced by decomposing trichlorid of anti?" mony with water,-jma beltreated {with mu. toarriveat quite tral glycolates in for er' similar products as bfo:

sodium or chlorid of calcium' fi'oni the p ucts produced accordingtotheprocessabbvd The herein described process of con- 100 ,compose even when diluted solution.

,- We claim described.- In place of oxy-chlorid of antimony also other antimony salts may be a plied, such as fiuorids or oxalates. Also t e meta-antimonic acid salts react with glycolic acid in the manner desired. Furthermore, solutions of acid glycolates are brought into reaction'with metallic antimony under theapplication of air, either by treating the powdered antimony in a shaking apparatus with solutions of acid glycolates, or. by passing a stream of air through a suspension of antimony powder in a solution of an acid glycolate, or by combiningboth processes.

Accordingto the above processes double salts may be produced, such as, for instance, potassium sodium glycolate of antimony, etc. For the production of antimony compounds the acid or neutral glycolic acid salts of alkalis and alkaline earth-metals are particularly well adapted.

The following example may give an approximate idea of the new process: 76 parts of glycolic acid are saturated in an aquepus solution with soda and 76 parts of glyoolic acid are added thereto. The solution is then heated to 70-80? C. and freshly. precipitated antimony oxid added thereto until dissolved. The solution is then filtered to remove the sli ht excess of antimony oxid and evaporated to ryness. In this manner about 300 parts of a crystalline product, capable of resisting the atmosphere, are obtained, which contain about 30% of antimony. f'"In order to obtain quantity of water, the solution obtained above is .once more mixed with about. the same quantit-y of acid sodiumglycolate, and

:themixture in solution is then evaporated to.-

i a product which is clearly soluble ina great dryness. In this manner about 480 parts of I a product are obtained which contains about 18% of antimony, and which does not deheated 'in a very much,

,{compound with a substance containing antimony.

verting a, g'l'y col ic acid compound into :1 names to this specification in the presence of mordant, which consists intreating said two subscribin witnesses.

compound with compounds of antimony. .OTTO IEBKNECHT.

3.v The herein described auxiliarymor-. V; FERDINAND; BLUMENTHAL. 5 dants, consisting of a compoundof glycolic Witnesses-ion both applicants acid and a substance containing antimony,- l Jm Grimm,

'In testimony whereof we have signed our CARL 'GRUND. 

